CN114833326A - Equipment and method for preparing eutectic high-temperature alloy by magnetic control electric arc and directional solidification - Google Patents

Equipment and method for preparing eutectic high-temperature alloy by magnetic control electric arc and directional solidification Download PDF

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CN114833326A
CN114833326A CN202210577534.5A CN202210577534A CN114833326A CN 114833326 A CN114833326 A CN 114833326A CN 202210577534 A CN202210577534 A CN 202210577534A CN 114833326 A CN114833326 A CN 114833326A
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dummy ingot
electric arc
water
dummy
ingot device
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CN114833326B (en
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陈瑞润
陈德志
王琪
王墅
王亮
苏彦庆
郭景杰
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Harbin Institute of Technology
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Harbin Institute of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/02Use of electric or magnetic effects
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D27/00Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
    • B22D27/04Influencing the temperature of the metal, e.g. by heating or cooling the mould
    • B22D27/045Directionally solidified castings
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B21/00Unidirectional solidification of eutectic materials
    • C30B21/02Unidirectional solidification of eutectic materials by normal casting or gradient freezing
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A device and a method for preparing eutectic high-temperature alloy by magnetic control electric arc directional solidification relate to a device and a method for high-temperature alloy directional solidification. The invention aims to solve the problems that in the prior art, the size of a sample is limited, continuous material supplement is difficult, a cooling medium is expensive, and the optimal directional solidification effect cannot be achieved due to the disturbance of electromagnetic induction heating on the front edge of a solid-liquid interface. The top of the dummy ingot device is contacted with the bottom of the water-cooled copper crucible, the spiral feeder is positioned above the side of the water-cooled copper crucible, and the top of the magnetic control device is connected with the inside of the vacuum furnace and sleeved outside the electric arc gun. Adjusting the current and frequency of the coil to values matched with the metal particles, keeping the values for 30s, reducing and stabilizing the arc action range, and controlling the magnetic control device to be discontinuously opened by the control cabinet; and simultaneously starting a control motor and a dummy ingot motor to supplement metal particles and grow and prepare the oriented structure. The method is used for preparing the high-temperature alloy.

Description

Equipment and method for preparing eutectic high-temperature alloy by magnetic control electric arc and directional solidification
Technical Field
The invention relates to equipment and a method for preparing eutectic high-temperature alloy directional solidification, in particular to equipment and a method for preparing eutectic high-temperature alloy directional solidification by a magnetic control electric arc. Belongs to the technical field of directional solidification of refractory eutectic alloy and metal-based composite alloy.
Background
The engine is the heart of the fighter plane, and the thrust-weight ratio of the engine is the key factor, wherein the material and the performance of the blade are the key factors. Most of the blade materials are metal and metal-based composite materials with the melting point of more than 2000 ℃, and the directional solidification is used as a main means for processing the blade, and is a method for regulating and controlling the alloy structure, reducing the transverse grain boundary and improving the comprehensive mechanical property of the alloy. However, the conventional directional solidification method can process a directional solidification sample with small size, is difficult to reach industrial size, and is expensive due to the adoption of liquid metal to provide a temperature gradient at the front edge of a solid-liquid interface. A part of heating modes, such as electromagnetic induction heating, can form strong convection at the front edge of a solid-liquid interface, so that the solid-liquid interface is a non-flat interface, and the directional solidification structure form of the alloy is influenced.
In conclusion, the size of a sample in the existing directionally solidified high-temperature alloy is limited, continuous material supplement is difficult during directional solidification of the high-temperature alloy, a liquid metal (indium liquid is added) cooling medium is expensive, and the problem that the best directional solidification effect cannot be achieved due to disturbance of electromagnetic induction heating on the front edge of a solid-liquid interface is solved.
Disclosure of Invention
The invention aims to solve the problems that the size of a sample in the existing directionally solidified high-temperature alloy is limited, materials are difficult to continuously supplement during directional solidification of the high-temperature alloy, a liquid metal cooling medium is expensive, and the optimal directional solidification effect cannot be achieved due to disturbance of electromagnetic induction heating on the front edge of a solid-liquid interface. Further provides equipment and a method for preparing the directional solidification of the eutectic high-temperature alloy by the magnetic control arc, so as to obtain the directional cast ingot of the eutectic high-temperature alloy, which has good coupling growth of a brittle phase and a toughness phase in the eutectic alloy and greatly improved fracture toughness.
The invention provides a high-frequency induction heating solidification device for preparing high-temperature alloy, which comprises a control cabinet, a connecting wire, an electric arc gun, a magnetic control device controller, a vacuum furnace, a spiral feeder, a control motor, a vacuum system, a magnetic control device, an electric arc gun, a water-cooled copper crucible, a dummy ingot system, a crucible and a dummy ingot device water inlet and outlet system, wherein the control cabinet is connected with the control cabinet; the water-cooled copper crucible is arranged in the vacuum furnace, the dummy ingot device system penetrates through the bottom end of the vacuum furnace and is connected with the lower part of the water-cooled copper crucible, the water inlet and outlet systems of the crucible and the dummy ingot device are arranged at the bottom of the water-cooled copper crucible and are used for cooling the water-cooled copper crucible and the dummy ingot device system, the spiral feeder is obliquely and hermetically inserted in the vacuum furnace towards the lower right side, the discharge end of the spiral feeder faces the water-cooled copper crucible, and the control motor is connected with the feed end of the spiral feeder and controls feeding; the vacuum system is arranged at the lower part of the outer side of the vacuum furnace to vacuumize the vacuum furnace, the electric arc gun is vertically inserted into the vacuum furnace and is positioned right above the water-cooled copper crucible, the magnetic control device is sleeved on the electric arc gun positioned in the vacuum furnace to change the depth of the electric arc gun for treating high-temperature alloy, the electric arc gun and the magnetic control device controller are arranged at the upper part of the electric arc gun, and the control cabinet is respectively and electrically connected with the control motor, the electric arc gun and the dummy ingot device system through connecting wires.
Further, the vacuum system comprises an air exhaust system and a protective gas input system, the air exhaust system is connected with the vacuum furnace through a pipeline, the protective gas input system is connected with the pipeline, and the protective gas introduced into the protective gas input system is argon.
Further, the magnetic control device comprises a magnetic conducting rod, a metal shielding cover, a coil and an I-shaped spiral pipe, the I-shaped spiral pipe is fixed on the inner side wall of the vacuum furnace through bolts, the coil is wound on the I-shaped spiral pipe, the metal shielding cover is covered on the outer side of the coil, the upper portion of the magnetic conducting rod is fixed on the I-shaped spiral pipe, and the bottom of the magnetic conducting rod is consistent with the bottom end of an electrode of the arc gun in height.
Further, the number of the magnetic conducting rods is four, the magnetic conducting rods comprise two long magnetic conducting rods and two short magnetic conducting rods, the top ends of the two long magnetic conducting rods are connected with the side face of the upper portion of the I-shaped solenoid through bolts, the two long magnetic conducting rods are symmetrically installed, the included angle is 180 degrees, the top ends of the two short magnetic conducting rods are connected with the side face of the lower portion of the I-shaped solenoid through bolts, the two short magnetic conducting rods are symmetrically installed, the included angle is 180 degrees, and the bottom ends of the four magnetic conducting rods are aligned with the tip end of the electric arc gun.
Furthermore, the crucible and dummy ingot device water inlet and outlet system comprises a water outlet pipe and a water inlet pipe, one end of the water outlet pipe and one end of the water inlet pipe are respectively inserted from two ends of the bottom of the water-cooled copper crucible to realize water cooling of the water-cooled copper crucible, and the other end of the water outlet pipe and the other end of the water inlet pipe are both connected with the dummy ingot device system to realize water cooling of the dummy ingot device system.
Furthermore, the dummy ingot device system comprises a dummy ingot device, a dummy ingot device sliding block, a dummy ingot device guide rail and a dummy ingot device motor, one end of the dummy ingot device penetrates through the vacuum furnace and then is connected with the lower end face of the water-cooled copper crucible, meanwhile, the upper portion of the dummy ingot device is connected with the crucible and the dummy ingot device water inlet and outlet system, the other end of the dummy ingot device is connected with the dummy ingot device sliding block, and the dummy ingot device motor drives the dummy ingot device sliding block to slide on the vertically installed dummy ingot device guide rail through a lead screw.
Furthermore, the dummy ingot device system also comprises a sealing device, and one end of the dummy ingot device is hermetically connected with the vacuum furnace through the sealing device.
The invention also provides a preparation method of the equipment for preparing the directional solidification of the eutectic high-temperature alloy by adopting the magnetic control electric arc, which comprises the following steps:
the method comprises the following steps: placing a seed crystal at the bottom of a water-cooled copper crucible, filling metal particles with the same components as the seed crystal in a spiral feeder, and descending and adjusting the electrode of an electric arc gun to the height capable of starting an arc;
step two: respectively setting the pull-down speed of the dummy bar and the dummy bar sliding block and the feeding amount of the spiral feeder on a control cabinet;
step three: starting a vacuum system, then starting an air exhaust system, introducing argon by using a protective gas input system, keeping the vacuum degree in the vacuum furnace at 0.05MPa, and striking an arc by using an arc gun;
step four: gradually increasing the arc current of the arc gun until the surface layer of the seed crystal is melted;
operating a magnetic control device, adjusting the current and the frequency of a coil to values matched with metal particles, reducing and keeping the range from the starting of the coil and the frequency to the electric arc action for 30s, reducing and stabilizing the electric arc action range, and controlling the magnetic control device to be discontinuously started by a control cabinet;
step five: simultaneously starting a control motor and a dummy ingot motor to supplement metal particles and grow directional tissues;
step six: after the preparation of the directional solidification cast ingot is finished, rapidly reducing the arc current to 0 within 1s-2s, and closing the current of an arc gun; after the directional cast ingot is completely cooled, starting an air exhaust system to exhaust air, opening a furnace door of the vacuum furnace and taking out the directional solidification cast ingot;
step seven: and performing wire cut electrical discharge machining on the directionally solidified eutectic ingot according to the standard of the engineering sample, polishing by using sand paper and a polishing machine, and then testing the structure and the mechanical property, thereby completing the preparation of the directionally solidified eutectic high-temperature alloy.
Further, in the second step, the pull-down speed range of the dummy ingot device and the dummy ingot device sliding block is 0-100mm/min, the feeding amount of the spiral feeder is matched with the pull-down speed of the dummy ingot device and the dummy ingot device sliding block, the conversion relation is that pi is multiplied by the seed crystal density multiplied by the square of seed crystal dendrite and multiplied by the pull-down speed of the dummy ingot device and the dummy ingot device sliding block, the conversion relation is integrated in the control cabinet, and only the pull-down speed of the dummy ingot device and the dummy ingot device sliding block is needed to be input.
Further, the electric arc of the electric arc gun in the fourth step enables the melting temperature of the surface layer of the seed crystal to be 100 ℃ on a liquid phase line, the current and the frequency of a coil of the magnetic control device are matched with the particle size of particles in the spiral feeder, the particle size is smaller than 100 micrometers, the current and the frequency of the coil are respectively controlled to be 50-100A and 50-100Hz, the particle size is larger than 100 micrometers, the current and the frequency of the coil are respectively controlled to be 100-200A and 30-50Hz, and the intermittent opening of the magnetic control device per second is staggered with the opening time of the spiral feeder.
Compared with the prior art, the invention has the following effects:
1. the equipment and the method for preparing the eutectic high-temperature alloy by adopting the magnetic control electric arc for directional solidification can carry out directional solidification preparation on the refractory eutectic alloy, simultaneously, the crucible is cooled by water, the cost of a directional solidification experiment is reduced, a spiral feeding device is adopted to realize the addition of continuous materials, simultaneously, the electric arc is adopted as a heating source, the influence on the shape of a solid-liquid boundary is small, the coupled directional growth of a brittle phase and a toughness phase in the eutectic alloy is realized, no pollution is caused, and the fracture toughness is greatly improved.
2. The invention adopts the magnetic control device to control the size and the action range of the electric arc, is convenient for the material addition of the spiral feeder, is not easy to blow away, simultaneously reduces the action depth of the electric arc, improves the large temperature gradient at the front edge of a solid-liquid interface, and is beneficial to the directional growth of eutectic alloy.
3. The ingot of the invention can reach industrial grade size:
the size of the water-cooled copper crucible is larger than 20mm, the size of seed crystals in the copper crucible can be adjusted according to needs, the diameter of the directional cast ingot mainly reaches the industrial grade, and the length of the directional cast ingot can be grown all the time according to feeding and the height of the crucible. Therefore, the ingot prepared by the invention can reach the industrial grade size.
4. The magnetic control device of the invention has the following specific functions:
(1) the magnetic control device changes the action depth of the electric arc from 1mm to 15mm by controlling the frequency and the current of the coil 803, changes the action depth of the electric arc, can change the temperature gradient in the directional solidification process, regulates the solid-liquid interface form, reduces the action depth of the electric arc, can increase the temperature gradient, is beneficial to the formation of a straight solid-liquid interface, is beneficial to the formation of a directional solidification structure, and improves the room-temperature fracture toughness of the cast ingot.
(2) The magnetic control device changes the action depth of the electric arc by controlling the frequency and the current of the coil 803, prevents the powder of the feeding from blowing away, ensures the amount of the added materials, and ensures the accuracy of the matching relationship of the feeding and the drawing.
(3) The magnetic control device changes the action depth of the electric arc by controlling the frequency and the current of the coil 803, is far away from the front edge of a solid-liquid interface, only smelts the surface of the seed crystal to form a larger temperature gradient, is more beneficial to forming a directional structure, and the good directional structure can obviously improve the axial mechanical property, particularly the room temperature fracture toughness, and is improved by 2.5 times.
5. The water-cooled copper crucible has the following advantages by adopting a water-cooling mode:
cold water flows in the crucible to provide a temperature gradient for directional solidification, most of other directional solidification temperature gradients are provided at the bottom by the GaIn liquid, the cost is very high, pollution is easy to generate, the pollution can be reduced by adopting the water-cooled copper crucible, and the water-cooled copper crucible is low in cost and easy to realize.
6. The invention can reduce the disturbance of the front edge of the solid-liquid interface:
in the directional solidification process, the form of a solid-liquid interface plays an important role in realizing the directional solidification growth of the cast ingot, the flat solid-liquid interface is more favorable for the directional solidification of the cast ingot, a directional tissue grows vertically to the solid-liquid interface, a single electric arc heating mode can have a powerful effect on a molten pool, the front edge of the solid-liquid interface is strongly disturbed, the directional solidification is not facilitated, and the action depth of an electric arc can be reduced and the disturbance in the molten pool can be reduced by the magnetic control added electric arc melting.
7. The drawing mechanism (ingot guiding device system) at the bottom of the invention plays a role:
the crucible and the seed crystal in the crucible move along with the pulling mechanism, so that the directional solidification process of the ingot is realized, the length of the ingot is not higher than that of the crucible, the whole magnetic control device can extend into the crucible deeply, and the whole magnetic control device is smaller than the inner diameter of the crucible. Therefore, the height of the ingot can be increased, the ingot can not penetrate into the crucible, the performance is not assisted, the height of the ingot is only consistent with that of the crucible, the ingot does not extend into the crucible, and the seed crystal cannot be melted.
8. The material prepared by the equipment has the advantages of improved performance:
in the present experiment, three groups of examples are provided with reference to fig. 4 to 6, and the performance improvement of the room temperature fracture toughness can be obviously improved by 2.5 times at most.
Drawings
FIG. 1 is a schematic structural diagram of a magnetron arc-based eutectic superalloy directional solidification apparatus of the present invention;
FIG. 2 is a partial cross-sectional view of A of FIG. 1;
FIG. 3 is a partial cross-sectional view of B of FIG. 1;
FIG. 4 shows Nb-Si-Ti-ZrC-TiB under scanning electron microscope 2 Directionally solidifying a structural picture by using an alloy magnetic control electric arc;
FIG. 5 shows Nb-Si-Ti-ZrC-TiB under scanning electron microscope 2 Directionally solidifying a structural picture by using an alloy magnetic control electric arc;
FIG. 6 is a graph of fracture toughness values for various examples.
Detailed Description
The first embodiment is as follows: the embodiment is described with reference to fig. 1 to 3, and comprises a control cabinet 1, a connecting wire 2, an electric arc gun and magnetic control device controller 3, a vacuum furnace 4, a spiral feeder 5, a control motor 6, a vacuum system 7, a magnetic control device 8, an electric arc gun 9, a water-cooled copper crucible 10, a dummy ingot system and crucible and dummy ingot device water inlet and outlet system 11; the water-cooled copper crucible 10 is arranged in the vacuum furnace 4, the dummy ingot device system passes through the bottom end of the vacuum furnace 4 and is connected with the lower part of the water-cooled copper crucible 10, the crucible and the dummy ingot device water inlet and outlet system 11 are arranged at the bottom of the water-cooled copper crucible 10 and are used for cooling the water-cooled copper crucible 10 and the dummy ingot device system, the spiral feeder 5 is obliquely and hermetically inserted in the vacuum furnace 4 towards the lower right side, the discharge end of the spiral feeder 5 faces the water-cooled copper crucible 10, and the control motor 6 is connected with the feed end of the spiral feeder 5 and controls feeding; the vacuum system 7 is arranged at the lower part of the outer side of the vacuum furnace 4 and used for vacuumizing the vacuum furnace 4, the electric arc gun 9 is vertically inserted into the vacuum furnace 4 and is positioned right above the water-cooled copper crucible 10, the magnetic control device 8 is sleeved on the electric arc gun 9 positioned in the vacuum furnace 4 to change the depth of the electric arc gun 9 for processing high-temperature alloy, the electric arc gun and magnetic control device controller 3 is arranged at the upper part of the electric arc gun 9, and the control cabinet 1 is respectively and electrically connected with the control motor 6, the electric arc gun 9 and the dummy ingot system through the connecting wire 2.
The control cabinet 1 of the present embodiment is used to control a power supply, a starter motor in a starter system, and a control motor of a screw feeder.
The electromagnetic field generated by the magnetic control device 8 of the embodiment generates acting force on the electric arc, so that the acting range and the acting depth of the electric arc can be reduced, the material addition of the spiral feeder is facilitated, and the disturbance of the front edge of a solid-liquid interface is reduced.
The feeding rod of the screw feeder 5 in the embodiment is driven by the control motor 6 to control the feeding speed, the feeding speed is controllable by adopting the method, the particle size of the fed material is not limited, the equipment is convenient to manufacture, and the operability is strong.
The method can carry out pollution-free directional solidification treatment on the refractory eutectic alloy, control the temperature gradient at the front edge of a solid-liquid interface by using the magnetic control device, control the feeding speed of the spiral feeder and the dummy ingot speed of the dummy ingot device, realize the directional growth of a melt structure, better obtain the refractory alloy directionally solidified ingot with the directionally grown structure, and further obtain the directionally solidified eutectic alloy with high mechanical property (ultrahigh room temperature fracture toughness).
The second embodiment is as follows: referring to fig. 1, the vacuum system 7 of the present embodiment includes an air extraction system 701 and a shielding gas input system 702, the air extraction system 701 is connected to the vacuum furnace 4 through a pipeline, and the shielding gas input system 702 is connected to the pipeline, wherein the shielding gas introduced into the shielding gas input system 702 is argon. So set up, be convenient for to the vacuum furnace evacuation and let in protective gas. Other components and connection modes are the same as those of the first embodiment.
The third concrete implementation mode: referring to fig. 2, the magnetic control apparatus 8 of the present embodiment includes a magnetic conducting rod 801, a metal shielding cover 802, a coil 803, and an i-shaped spiral pipe 804, the i-shaped spiral pipe 804 is fixed on the inner side wall of the vacuum furnace 4 by bolts, the coil 803 is wound on the i-shaped spiral pipe 804, the metal shielding cover 802 covers the outer side of the coil 803, the upper portion of the magnetic conducting rod 801 is fixed on the i-shaped spiral pipe 804, and the bottom of the magnetic conducting rod 801 is at the same height as the bottom end of the electrode of the arc gun 9. (the arc gun 9 can be moved up and down by the arc gun and the magnetron controller, and is shown in FIG. 2 without adjustment). So set up, the size and the application range of control electric arc, the material of the screw feeder of being convenient for adds, and is difficult for blowing to fly, reduces the depth of action of electric arc simultaneously, for the leading edge improvement big temperature gradient of solid-liquid interface, is favorable to the directional growth of eutectic alloy. Other components and connection modes are the same as those of the first embodiment or the second embodiment.
The fourth concrete implementation mode: referring to fig. 2, the embodiment is described, the number of the magnetic conduction rods 801 of the embodiment is four, and the magnetic conduction rods include two long magnetic conduction rods and two short magnetic conduction rods, the top ends of the two long magnetic conduction rods are connected with the side surface of the upper portion of the i-shaped solenoid 804 through bolts, the two long magnetic conduction rods are symmetrically installed, an included angle is 180 degrees, the top ends of the two short magnetic conduction rods are connected with the side surface of the lower portion of the i-shaped solenoid 804 through bolts, the two short magnetic conduction rods are symmetrically installed, the included angle is 180 degrees, and the bottom ends of the four magnetic conduction rods 801 are all aligned with the tip end of the arc gun 9. By the arrangement, the electromagnetic force generated by the magnetic control device acts on the top of the arc, so that the shape of the arc is better controlled. Other components and connection modes are the same as those of the first, second or third embodiment modes.
The fifth concrete implementation mode: referring to fig. 1 and fig. 3, the crucible and dummy ingot inlet and outlet water system 11 of the present embodiment includes a water outlet pipe 1101 and a water inlet pipe 1102, wherein one end of the water outlet pipe 1101 and one end of the water inlet pipe 1102 are respectively inserted into two ends of the bottom of the water-cooled copper crucible 10 to realize water cooling of the water-cooled copper crucible 10, and the other end of the water outlet pipe 1101 and the other end of the water inlet pipe 1102 are both connected to the dummy ingot system to realize water cooling of the dummy ingot system. So set up, be convenient for cool off water-cooling copper crucible and dummy ingot ware. Other components and connection modes are the same as those of the first, second, third or fourth embodiment modes.
The sixth specific implementation mode: the present embodiment is described with reference to fig. 3, and the dummy ingot device system of the present embodiment includes a dummy ingot device 12, a dummy ingot device slider 14, a dummy ingot device guide rail 13, and a dummy ingot device motor 15, wherein one end of the dummy ingot device 12 is connected to the lower end surface of the water-cooled copper crucible 10 after passing through the vacuum furnace 4, meanwhile, the upper portion of the dummy ingot device 12 is connected to the crucible and the dummy ingot device water inlet and outlet system 11, the other end of the dummy ingot device 12 is connected to the dummy ingot device slider 14, and the dummy ingot device motor 15 drives the dummy ingot device slider 14 to slide on the vertically installed dummy ingot device guide rail 13 through a lead screw. So set up, be convenient for realize the directional solidification process of ingot casting, the ingot casting height has reached the height of water-cooling copper crucible. Other components and connection modes are the same as those of the first, second, third, fourth or fifth embodiment modes.
The seventh embodiment: the embodiment is described with reference to fig. 3, the dummy ingot system of the embodiment further includes a sealing device 17, one end of the dummy ingot 12 is connected with the vacuum furnace 4 through the sealing device 17 in a sealing manner, wherein the sealing device 17 includes a threaded connection portion and a sealing portion, the threaded connection portion is connected with the bottom of the vacuum furnace 4 through the dummy ingot 12 of the dummy ingot system, the sealing portion is a sealing gasket, a sealing vacuum grease is coated on the external sealing portion of the vacuum furnace 4, the material of the sealing device is the same as that of the vacuum furnace 4, the sealing gasket is made of steel, and the material of the sealing gasket is rubber. So set up, because dummy ingot system's motion can reduce vacuum chamber's leakproofness, consequently increase sealing device and carry out better sealed, guarantee the vacuum. Other components and connection modes are the same as those of the first, second, third, fourth, fifth or sixth embodiment.
The specific implementation mode is eight: the present embodiment will be described with reference to fig. 1 to 3, and the preparation method of the present embodiment is characterized in that: it comprises the following steps:
the method comprises the following steps: placing a seed crystal 16 at the bottom of a water-cooled copper crucible 10, filling the screw feeder 5 with metal particles of the same composition as the seed crystal, and lowering and adjusting the electrode of an electric arc gun 9 to a height capable of starting an arc;
step two: respectively setting the pull-down speed of a dummy bar 12 and a dummy bar sliding block 14 and the feeding amount of the screw feeder 5 on the control cabinet 1;
step three: starting the vacuum system 7, then starting the gas extraction system 701, filling argon gas by using the protective gas input system 702, keeping the vacuum degree in the vacuum furnace 4 at 0.05MPa, and striking an arc by using the arc gun 9;
step four: gradually increasing the arc current of the arc gun 9 until the surface layer of the seed crystal 16 is melted;
the magnetic control device 8 is operated, the current and the frequency of the coil 803 are adjusted to be values matched with metal particles, the range from the opening of the coil and the frequency to the action of the electric arc is reduced and kept for 30s, the action range of the electric arc is reduced and stabilized because the magnetic control device adjusts the time required for searching the frequency and increasing the current, and the magnetic control device 8 is controlled by the control cabinet 1 to be opened discontinuously;
step five: simultaneously starting a control motor 6 and a dummy ingot motor 15 to supplement metal particles and grow directional tissues;
step six: after the preparation of the directional solidification cast ingot is finished, rapidly reducing the arc current to 0 within 1s-2s, and closing the current of the arc gun 9; after the directional cast ingot is completely cooled, starting an air extraction system 701 to deflate, opening a furnace door of a vacuum furnace 4 and taking out the directional solidification cast ingot;
step seven: and performing wire cut electrical discharge machining on the directionally solidified eutectic ingot according to the standard of the engineering sample, polishing by using sand paper and a polishing machine, and then testing the structure and the mechanical property, thereby completing the preparation of the directionally solidified eutectic high-temperature alloy.
The specific implementation method nine: referring to fig. 1 to 3, the pulling-down speed of the dummy bar 12 and the dummy bar slider 14 in the second step of the present embodiment is in the range of 0-100mm/min, the feeding amount of the screw feeder 5 is matched with the pulling-down speed of the dummy bar 12 and the dummy bar slider 14, and the conversion relationship is pi multiplied by the seed crystal density multiplied by the square of the seed crystal dendrite and multiplied by the pulling-down speed of the dummy bar 12 and the dummy bar slider 14, which has been integrated in the control cabinet 1, and only the pulling-down speed of the dummy bar 12 and the dummy bar slider 14 needs to be input. So set up, guarantee the supply of directional solidification in-process material, reduce the defect of ingot casting. Other components and connection modes are the same as those of any one of the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment is described with reference to fig. 1 to 3, the arc of the arc gun 6 in the fourth step of the present embodiment enables the melting temperature of the surface layer of the seed crystal 16 to be 100 ℃ on the liquidus line, the current and frequency of the coil 803 of the magnetic control device 8 are matched with the particle size of the particles in the screw feeder 5, the particle size is less than 100 μm, the current and frequency of the coil 803 are respectively controlled to be 50-100A and 50-100Hz, the particle size is greater than 100 μm, the current and frequency of the coil 803 are respectively controlled to be 100A and 30-50Hz, and the intermittent opening of the magnetic control device 8 per second is staggered with the opening time of the screw feeder 5. So set up, open time staggers, when adding the material, guarantees that the granule is not blown to fly away, can make the granule melt better simultaneously. The other components and the connection mode are the same as those of the ninth embodiment.
Example 1:
Nb-Si-Ti-ZrC-TiB prepared by using magnetic control electric arc of equipment 2 The method for directionally casting the eutectic alloy ingot comprises the following steps:
step 1: a seed crystal 16, having a diameter of 20mm, was placed at the bottom of the water-cooled copper crucible 10, and the screw feeder was filled with metal particles of the same composition as the seed crystal. The particle size is 80 μm, and the electrode of the arc gun 9 is lowered and adjusted to a height capable of striking an arc;
step 2: setting the pull-down speed of a dummy ingot device 12 and a dummy ingot device sliding block 14 and the feeding quantity of a spiral feeder 5 to be 100mm/min and 3.9g/s on a power supply, the dummy ingot device and the spiral feeder control cabinet 1 respectively;
and step 3: starting the vacuum system 7, then starting the gas extraction system 701, filling argon gas by using the protective gas input system 702, keeping the vacuum degree in the vacuum furnace 4 at 0.05MPa, and striking an arc by using the arc gun 9;
and 4, step 4: gradually increasing the arc current of the arc gun 9 until the surface layer of the seed crystal 16 is melted at 600A;
operating the magnetic control device 8, adjusting the current and the frequency of the coil 803 to 80A and 80Hz, keeping for 30s, reducing and stabilizing the arc action range, and controlling the magnetic control device 8 to be discontinuously opened by a power supply, a dummy ingot device and the spiral feeder control cabinet 1;
and 5: simultaneously starting the control motor 6 and the dummy ingot motor 15 to supplement metal particles and grow directional tissues
Step 6: after the preparation of the directional solidification cast ingot is finished, reducing the electric arc current to 0 within 1s, after the directional cast ingot is completely cooled, starting an air extraction system 701 to deflate, opening a furnace door of a vacuum furnace 4 and taking out the directional solidification cast ingot.
And 7: and performing wire cut electrical discharge machining on the directionally solidified eutectic cast ingot according to the standard of the engineering sample, and performing texture and fracture toughness tests after polishing and burnishing by using sand paper and a burnishing machine.
Example 2:
the Nb-Si-Ti-ZrC-TiB is prepared by using the magnetic control electric arc of the equipment 2 The method for directionally casting the eutectic alloy ingot comprises the following steps:
step 1: a seed crystal 16, having a diameter of 30mm, was placed at the bottom of the water-cooled copper crucible 10, and the screw feeder was filled with metal particles of the same composition as the seed crystal. The particle size is 120 μm, and the electrode of the arc gun 9 is lowered and adjusted to a height capable of striking an arc;
step 2: setting the pull-down speed of the dummy ingot device 12 and the dummy ingot device sliding block 14 and the feeding quantity of the spiral feeder 5 to be 80mm/min and 6.9g/s on the power supply, the dummy ingot device and the spiral feeder control cabinet 1 respectively;
and step 3: starting the vacuum system 7, then starting the gas extraction system 701, filling argon gas by using the protective gas input system 702, keeping the vacuum degree in the vacuum furnace 4 at 0.05MPa, and striking an arc by using the arc gun 9;
and 4, step 4: gradually increasing the arc current of the arc gun 9 until the surface layer of the seed crystal 16 is melted at 600A;
operating the magnetic control device 8, adjusting the current and the frequency of the coil 803 to 150A and 40Hz, keeping the current and the frequency for 30s, reducing and stabilizing the arc action range, and controlling the magnetic control device 8 to be discontinuously opened by a power supply, a dummy ingot device and the spiral feeder control cabinet 1;
and 5: simultaneously starting the control motor 6 and the dummy ingot motor 15 to supplement metal particles and grow directional tissues
Step 6: after the preparation of the directional solidification cast ingot is finished, reducing the electric arc current to 0 within 1s, after the directional cast ingot is completely cooled, starting an air extraction system 701 to deflate, opening a furnace door of a vacuum furnace 4 and taking out the directional solidification cast ingot.
And 7: and performing wire cut electrical discharge machining on the directionally solidified eutectic cast ingot according to the standard of the engineering sample, and performing texture and fracture toughness tests after polishing and burnishing by using sand paper and a burnishing machine.
Example 3:
a method for preparing an Nb-Si-Ti-ZrC-Sc eutectic alloy oriented ingot by using the magnetic control electric arc of the equipment comprises the following steps:
step 1: a seed crystal 16, having a diameter of 32mm, was placed at the bottom of a water-cooled copper crucible 10, and the screw feeder was filled with metal particles of the same composition as the seed crystal. The particle size is 60 μm, and the electrode of the arc gun 9 is lowered and adjusted to a height capable of striking an arc;
step 2: respectively setting the pull-down speed of a dummy ingot device 12 and a dummy ingot device sliding block 14 and the feeding quantity of a spiral feeder 5 to be 90mm/min and 8.9g/s on a power supply, the dummy ingot device and the spiral feeder control cabinet 1;
and step 3: starting the vacuum system 7, then starting the gas extraction system 701, filling argon gas by using the protective gas input system 702, keeping the vacuum degree in the vacuum furnace 4 at 0.05MPa, and striking an arc by using the arc gun 9;
and 4, step 4: gradually increasing the arc current of the arc gun 9 until the 650A seed crystal 16 surface layer is melted;
operating the magnetic control device 8, adjusting the current and the frequency of the coil 803 to 70A and 80Hz, keeping for 30s, reducing and stabilizing the arc action range, and controlling the magnetic control device 8 to be discontinuously opened by a power supply, a dummy ingot device and the spiral feeder control cabinet 1;
and 5: simultaneously starting the control motor 6 and the dummy ingot motor 15 to supplement metal particles and grow directional tissues
Step 6: after the preparation of the directional solidification cast ingot is finished, reducing the electric arc current to 0 within 2s, after the directional cast ingot is completely cooled, starting an air extraction system 701 to deflate, opening a furnace door of a vacuum furnace 4 and taking out the directional solidification cast ingot.
And 7: and performing wire cut electrical discharge machining on the directionally solidified eutectic cast ingot according to the standard of the engineering sample, and performing texture and fracture toughness tests after polishing and burnishing by using sand paper and a burnishing machine.
FIG. 4 shows Nb-Si-Ti-ZrC-TiB under scanning electron microscope 2 Preparing a texture picture by alloy directional solidification; the microstructure has obvious orientation effect, comprises silicide phase with relatively large size and Nbss eutectic structure, and also comprises dendritic silicide with fine size and Nbss eutectic structure. FIG. 4 shows the preparation of Nb-Si-Ti-ZrC-TiB by magnetic control arc in the embodiment of the invention 2 The alloy microstructure shows that the Nb-Si prepared by the magnetic control electric arc preparation device and the method-Ti-ZrC-TiB 2 The microstructure in the alloy obviously appears directional arrangement growth, and a fine dendritic eutectic structure exists, wherein the size of dendritic eutectic clusters of the cast ingot in the figure is 10-20 mu m mostly. The good oriented structure in the structure improves the room temperature fracture toughness and is formed by the cast state of 13 MPa.m 1/2 30 MPa.m for increasing to directional solidification state 1/2 . Therefore, the alloy prepared by the magnetic control electric arc can realize the directional growth of the cast ingot and improve the mechanical property of the alloy.
FIG. 5 shows Nb-Si-Ti-ZrC-TiB prepared by magnetic control arc under scanning electron microscope 2 The alloy structure picture has obvious structure orientation effect. FIG. 5 shows the preparation of Nb-Si-Ti-ZrC-TiB by magnetic control arc in the embodiment of the invention 2 The alloy microstructure shows that the Nb-Si-Ti-ZrC-TiB prepared by the magnetic control arc device and the method of the invention 2 The microstructure in the alloy apparently grew directionally, with the average size of the black primary phase being about 4 μm and the average size of the white Nbss phase being about 2 μm. Wherein, a great amount of dendritic eutectic structures appear in the structure, the good oriented structure in the structure improves the room temperature fracture toughness, and the cast state of the structure is 13 MPa.m 1/2 Is increased to 28 MPa.m 1/2 . Therefore, the alloy prepared by the magnetic control electric arc can obviously enable the structure to grow directionally, and improve the room-temperature mechanical property of the alloy.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. The equipment for preparing the eutectic high-temperature alloy by the magnetic control electric arc is characterized in that: the device comprises a control cabinet (1), a connecting wire (2), an electric arc gun and magnetic control device controller (3), a vacuum furnace (4), a spiral feeder (5), a control motor (6), a vacuum system (7), a magnetic control device (8), an electric arc gun (9), a water-cooled copper crucible (10), an ingot starter system, a crucible and ingot starter water inlet and outlet system (11);
the water-cooled copper crucible (10) is arranged in the vacuum furnace (4), the dummy ingot device system penetrates through the bottom end of the vacuum furnace (4) and is connected with the lower part of the water-cooled copper crucible (10), the crucible and the dummy ingot device water inlet and outlet system (11) are arranged at the bottom of the water-cooled copper crucible (10) and are used for cooling the water-cooled copper crucible (10) and the dummy ingot device system, the spiral feeder (5) is obliquely and hermetically inserted into the vacuum furnace (4) towards the lower right side, the discharge end of the spiral feeder (5) faces towards the water-cooled copper crucible (10), and the control motor (6) is connected with the feed end of the spiral feeder (5) and controls feeding; the vacuum system (7) is installed on the lower portion of the outer side of the vacuum furnace (4) and used for vacuumizing the vacuum furnace (4), the electric arc gun (9) is vertically inserted into the vacuum furnace (4) and located right above the water-cooled copper crucible (10), the magnetic control device (8) is sleeved on the electric arc gun (9) located in the vacuum furnace (4) to change the depth of the electric arc gun (9) for processing high-temperature alloy, the electric arc gun and the magnetic control device controller (3) are installed on the upper portion of the electric arc gun (9), and the control cabinet (1) is electrically connected with the control motor (6), the electric arc gun (9) and the ingot starter system through the connecting wires (2).
2. The apparatus of claim 1, wherein the apparatus comprises: the vacuum system (7) comprises an air extraction system (701) and a protective gas input system (702), the air extraction system (701) is connected with the vacuum furnace (4) through a pipeline, the protective gas input system (702) is connected with the pipeline, and the protective gas introduced into the protective gas input system (702) is argon.
3. The apparatus of claim 2, wherein the apparatus comprises: the magnetic control device (8) comprises a magnetic conducting rod (801), a metal shielding cover (802), a coil (803) and an I-shaped spiral pipe (804), the I-shaped spiral pipe (804) is fixed on the inner side wall of the vacuum furnace (4) through a bolt, the coil (803) is wound on the I-shaped spiral pipe (804), the metal shielding cover (802) covers the outer side of the coil (803), the upper portion of the magnetic conducting rod (801) is fixed on the I-shaped spiral pipe (804), and the bottom of the magnetic conducting rod (801) is consistent with the bottom end height of an electrode of the electric arc gun (9).
4. The apparatus of claim 3, wherein the apparatus comprises: the number of the magnetic conducting rods (801) is four, the magnetic conducting rods comprise two long magnetic conducting rods and two short magnetic conducting rods, the top ends of the two long magnetic conducting rods are connected with the side face of the upper portion of the I-shaped solenoid (804) through bolts, the two long magnetic conducting rods are symmetrically installed, the included angle is 180 degrees, the top ends of the two short magnetic conducting rods are connected with the side face of the lower portion of the I-shaped solenoid (804) through bolts, the two short magnetic conducting rods are symmetrically installed, the included angle is 180 degrees, and the bottom ends of the four magnetic conducting rods (801) are all aligned with the tip end of the electric arc gun (9).
5. The apparatus for preparing eutectic superalloy directional solidification by magnetron arc according to claim 1 or 4, wherein: the crucible and dummy ingot device water inlet and outlet system (11) comprises a water outlet pipe (1101) and a water inlet pipe (1102), one end of the water outlet pipe (1101) and one end of the water inlet pipe (1102) are respectively inserted from two ends of the bottom of the water-cooled copper crucible (10) to realize water cooling of the water-cooled copper crucible (10), and the other end of the water outlet pipe (1101) and the other end of the water inlet pipe (1102) are both connected with a dummy ingot device system to realize water cooling of the dummy ingot device system.
6. The apparatus of claim 5, wherein the apparatus comprises: the dummy ingot device system comprises a dummy ingot device (12), a dummy ingot device sliding block (14), a dummy ingot device guide rail (13) and a dummy ingot device motor (15), one end of the dummy ingot device (12) penetrates through the vacuum furnace (4) and then is connected with the lower end face of the water-cooled copper crucible (10), meanwhile, the upper portion of the dummy ingot device (12) is connected with the crucible and a dummy ingot device water inlet and outlet system (11), the other end of the dummy ingot device (12) is connected with the dummy ingot device sliding block (14), and the dummy ingot device motor (15) drives the dummy ingot device sliding block (14) to slide on the vertically installed dummy ingot device guide rail (13) through a lead screw.
7. The apparatus of claim 6, wherein the apparatus comprises: the dummy ingot device system also comprises a sealing device (17), and one end of the dummy ingot device (12) is hermetically connected with the vacuum furnace (4) through the sealing device (17).
8. A method of manufacturing an apparatus for directional solidification of eutectic superalloy using a magnetron arc as claimed in any of claims 1 to 7, wherein: it comprises the following steps:
the method comprises the following steps: placing a seed crystal (16) at the bottom of a water-cooled copper crucible (10), filling a screw feeder (5) with metal particles with the same components as the seed crystal, and descending and adjusting the electrode of an electric arc gun (9) to the height capable of starting an arc;
step two: respectively setting the pull-down speed of a dummy bar (12) and a dummy bar sliding block (14) and the feeding amount of a spiral feeder (5) on a control cabinet (1);
step three: starting a vacuum system (7), then starting an air extraction system (701), filling argon by using a protective gas input system (702), keeping the vacuum degree in the vacuum furnace (4) at 0.05MPa, and striking an arc by using an arc gun (9);
step four: gradually increasing the arc current of the arc gun (9) until the surface layer of the seed crystal (16) is melted;
operating a magnetic control device (8), adjusting the current and the frequency of the coil (803) to values matched with metal particles, reducing and keeping the range from the coil opening and the frequency to the arc action for 30s, reducing and stabilizing the arc action range, and controlling the magnetic control device (8) to be opened discontinuously by a control cabinet (1);
step five: simultaneously starting a control motor (6) and a dummy ingot motor (15) to supplement metal particles and grow directional tissues;
step six: after the preparation of the directional solidification cast ingot is finished, quickly reducing the arc current to 0 within 1s-2s, and closing the current of an arc gun (9); after the directional cast ingot is completely cooled, starting an air extraction system (701) to deflate, opening a furnace door of the vacuum furnace (4) and taking out the directional solidification cast ingot;
step seven: and performing wire cut electrical discharge machining on the directionally solidified eutectic ingot according to the standard of the engineering sample, polishing by using sand paper and a polishing machine, and then testing the structure and the mechanical property, thereby completing the preparation of the directionally solidified eutectic high-temperature alloy.
9. The method of claim 8, wherein: in the second step, the pull-down speed range of the dummy ingot device (12) and the dummy ingot device sliding block (14) is 0-100mm/min, the feeding amount of the spiral feeder (5) is matched with the pull-down speed of the dummy ingot device (12) and the dummy ingot device sliding block (14), and the conversion relation is that pi is multiplied by the seed crystal density multiplied by the square of seed crystal dendrite and multiplied by the pull-down speed of the dummy ingot device (12) and the dummy ingot device sliding block (14), the conversion relation is integrated in the control cabinet (1), and only the pull-down speed of the dummy ingot device (12) and the dummy ingot device sliding block (14) needs to be input.
10. The method for producing according to claim 9, characterized in that: and fourthly, the electric arc of the electric arc gun (6) enables the melting temperature of the surface layer of the seed crystal (16) to be 100 ℃ on a liquid phase line, the current and the frequency of a coil (803) of the magnetic control device (8) are matched with the particle size of the particles in the spiral feeder (5), the particle size of the particles is smaller than 100 mu m, the current and the frequency of the coil (803) are respectively controlled to be 50-100A and 50-100Hz, the particle size of the particles is larger than 100 mu m, the current and the frequency of the coil (803) are respectively controlled to be 100-200A and 30-50Hz, and the intermittent opening of the magnetic control device (8) per second is staggered with the opening time of the spiral feeder (5).
CN202210577534.5A 2022-05-25 2022-05-25 Device and method for preparing eutectic superalloy directional solidification by magnetic control electric arc Active CN114833326B (en)

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